分散液液微萃取-气相色谱-串联质谱法检测水中十种有机氯农药  

Determination of 10 organochlorine pesticides in water by dispersive liquid-liquid microextraction coupled with GC-MS/MS

作　　者：袁悦 任琳[1] 江阳[1] 雍莉[1] YUAN Yue;REN Lin;JIANG Yang;YONG Li(Center of Disease Control and Prevention for Sichuan,Chengdu,Sichuan 610041,China)

机构地区：[1]四川省疾病预防控制中心,四川成都610041

出　　处：《现代预防医学》2023年第16期3043-3047,共5页Modern Preventive Medicine

摘　　要：目的建立水中十氯酮等10种有机氯农药的分散液液微萃取-气相色谱-串联质谱分析方法。方法将400μl萃取剂二硫化碳(含内标,浓度均为100μg/L)加入10 ml水样中,加入400μl分散剂丙酮并涡旋促进乳化分散;加入2g氯化钠,涡旋溶解以促进分层;离心后,弃去上层水相,取下层有机相进样分析。采用DB-5MS UI毛细管色谱柱程序升温分离,多反应监测模式检测,内标校正标准曲线法定量。结果方法在10~200μg/L范围内线性良好,方法检出限范围为1.48~58.7 ng/L,加标回收率为66.7%~138%,相对标准偏差为1.48%~12.9%。结论该方法前处理简单高效、检测灵敏准确,适用于水样中十种有机氯农药的快速测定。Objective To establish a dispersive liquid-liquid microextraction coupled with gas chromatography-tandem mass spectrometry method for the analysis of the 10 organochlorine pesticides including chlordecone in water samples.Methods 400μl of carbon disulfide(containing 100μg/L internal standards)as extractant was added into 10 ml water sample.The mixture was emulsified and dispersed with 400μl of acetone as dispersant by vortex mixing.Then,2 g sodium chloride was added and vortexed until dissolved to promote stratification.After centrifugation,the upper aqueous phase was discarded,and the organic phase was collected for further analysis.Gas chromatographic separation was achieved on a DB-5MS UI capillary column with temperature programming.Multiple reaction monitoring was used in mass spectrometric analysis and quantitative analysis was completed by internal standard method.Results The linear ranges of the method were from 10 to 200μg/L.The method detection limits were 1.48-58.7 ng/L.The average recoveries of the method were ranged from 66.7% to 138%,with the relative standard derivations between 1.48% and 12.9%.Conclusion The proposed method is simple,efficient,sensitive.It is suitable for the rapid determination of 10 organochlorine pesticides in water samples.

关 键 词：十氯酮 有机氯农药 水 分散液液微萃取 GC-MS/MS 

分 类 号：R123.1[医药卫生—环境卫生学]